CN103012676A - Preparation method of alkalescent TAIC (Triallyl isocyanurate) anion exchange resin - Google Patents

Preparation method of alkalescent TAIC (Triallyl isocyanurate) anion exchange resin Download PDF

Info

Publication number
CN103012676A
CN103012676A CN2012104898838A CN201210489883A CN103012676A CN 103012676 A CN103012676 A CN 103012676A CN 2012104898838 A CN2012104898838 A CN 2012104898838A CN 201210489883 A CN201210489883 A CN 201210489883A CN 103012676 A CN103012676 A CN 103012676A
Authority
CN
China
Prior art keywords
water
exchange resin
preparation
taic
warming
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2012104898838A
Other languages
Chinese (zh)
Other versions
CN103012676B (en
Inventor
姚能平
梅德华
***
林伟
王海宽
王玉兰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Wandong Chemical Co Ltd
Original Assignee
Anhui Wandong Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Wandong Chemical Co Ltd filed Critical Anhui Wandong Chemical Co Ltd
Priority to CN201210489883.8A priority Critical patent/CN103012676B/en
Publication of CN103012676A publication Critical patent/CN103012676A/en
Application granted granted Critical
Publication of CN103012676B publication Critical patent/CN103012676B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Phenolic Resins Or Amino Resins (AREA)

Abstract

The invention discloses a preparation method of alkalescent TAIC (Triallyl isocyanurate) anion exchange resin. On the basis of the traditional production process, the preparation method disclosed by the invention has the characteristics that a suspension protection agent, a dispersing agent, a pore-forming agent and a complexing agent are reasonably matched, and the process parameters are optimized, so that the anion exchange resin prepared by using the preparation method is uniform in pore diameter distribution and increased in exchange capacity; and the specific surface area of the prepared ion exchange resin is more than 70m<2>/g, the proportion of mesopores which are larger than 2nm is larger than 50 percent and the complete exchange capacity reaches 9.8mmol/g.

Description

The preparation method of weakly alkaline TAIC anionite-exchange resin
Technical field
The invention belongs to a kind of preparation method of ion exchange resin, specifically a kind of preparation method of weakly alkaline TAIC anionite-exchange resin.
Background technology
Anion and cation exchange resin is widely used for the fields such as the decolouring of the purification of water treatment, material, concentrated, separation, transformation that substance ion forms, material and catalyzer.Although the exchange capacity of present anion and cation exchange resin has obtained effective raising, pore size distribution is uneven, and the aperture ratio is excessive, and exchange velocity is low.The problems such as exchange capacity deficiency do not satisfy client's requirement.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of weakly alkaline TAIC anionite-exchange resin, the present invention are by the improvement of water, so that dispersed, suspension raising, and then reach the exchange capacity that increases ion exchange resin, the effect of even aperture distribution.
Technical scheme of the present invention is as follows:
The preparation method of weakly alkaline TAIC anionite-exchange resin is characterized in that may further comprise the steps:
(1), polymerization prepares A material, may further comprise the steps:
Figure 778179DEST_PATH_IMAGE002
The water raw material that takes by weighing following weight part mixes, and stirs;
Deionized water 500-600
Gelatin 30-35
Walocel MT 20.000PV 50-60
Quadrol 15-20
Sodium-chlor 80-85
Sodium Persulfate 1-2
Be neutral with sulfuric acid water transfer phase PH
Take by weighing the raw material of following weight part, aqueous phase after adding after mixing is adjusted rotating speed depending on the granularity situation;
Methyl acrylate 32-34
Divinylbenzene 50-55
TAIC 270-290
200# gasoline 158-163
Clorafin 50-55
Ferrocene 8-12
Diisopropyl azodicarboxylate 3-5
Figure 220979DEST_PATH_IMAGE006
Slowly be warming up to 65-69 ℃, note observing spheroid granularity and typing situation;
Figure 828546DEST_PATH_IMAGE008
Heat release during typing, cooling maintains the temperature at 68-70 ℃ after the heat release, be incubated 2-3 hour;
Figure 428679DEST_PATH_IMAGE010
Be warming up to 80-82 ℃ of insulation 3-4h with the 25-40 minutes;
Figure 479812DEST_PATH_IMAGE012
With 92-96 ℃ of insulation of 50-70 minutes intensification 4-5h;
Figure 591993DEST_PATH_IMAGE014
With the hot water wash nodule number all over till limpid to water;
Figure 753984DEST_PATH_IMAGE016
Drain water, oven dry, sub-sieve makes the A material.
(2), amination reaction prepares the B material
Figure 2432DEST_PATH_IMAGE002
Press the row weight part and take by weighing following raw materials according, in clean reactor, add A material and tetraethylene pentamine, start stirring;
A expects 380-420
Tetraethylene pentamine 1580-1620
Figure 411417DEST_PATH_IMAGE004
Be warming up to 130-135 ℃, insulation reaction 15-18h, the control exchange is qualified greater than 8.0mmol/g in the survey;
Figure 761627DEST_PATH_IMAGE006
After middle control is qualified, take out mother liquor, reclaim tetraethylene pentamine;
Figure 997084DEST_PATH_IMAGE008
Massive laundering is drained to neutral, gets the B material;
(3), methylation reaction prepares resin
2, operation steps
Figure 303300DEST_PATH_IMAGE002
The B material is added in the mixing raw material of following weight part, start stirring;
Formic acid 1150-1250
Water 200-240
Formaldehyde 60-65
Oxalic acid 50-55
Be warming up to 48-50 ℃, kept 20-40 minute;
Figure 517430DEST_PATH_IMAGE006
Drain mother liquor, massive laundering is drained discharging to neutral.
The present invention is by reasonably combined suspension protective material, dispersion agent, pore-creating agent, complexing agent; Optimizing Process Parameters, so that the anionite-exchange resin of present method preparation, even aperture distribution; the effect that exchange capacity improves, the ion exchange resin specific surface area that the present invention makes can reach 70m 2More than/the g, greater than 50%, complete exchange capacity reaches 11.8mmol/g greater than the mesopore ratio of 2nm.
Embodiment
The preparation method of weakly alkaline TAIC anionite-exchange resin may further comprise the steps:
(1), polymerization prepares A material, may further comprise the steps:
Figure 21224DEST_PATH_IMAGE002
The water raw material that takes by weighing following weight (kilogram) mixes, and stirs;
Deionized water 500
Gelatin 30
Walocel MT 20.000PV 50
Quadrol 15
Sodium-chlor 80
Sodium Persulfate 1
Be neutral with sulfuric acid water transfer phase PH
Figure 447526DEST_PATH_IMAGE004
Take by weighing the raw material of following weight (kilogram), aqueous phase after adding after mixing is adjusted rotating speed depending on the granularity situation;
Methyl acrylate 32
Divinylbenzene 50
TAIC 270
200# gasoline 158
Clorafin 50
Ferrocene 8
Diisopropyl azodicarboxylate 3
Figure 997980DEST_PATH_IMAGE006
Slowly be warming up to 65-69 ℃, note observing spheroid granularity and typing situation;
Figure 322782DEST_PATH_IMAGE008
Heat release during typing, cooling maintains the temperature at 68-70 ℃ after the heat release, be incubated 2-3 hour;
Be warming up to 80-82 ℃ of insulation 3-4h with the 25-40 minutes;
Figure 707813DEST_PATH_IMAGE012
With 92-96 ℃ of insulation of 50-70 minutes intensification 4-5h;
With the hot water wash nodule number all over till limpid to water;
Figure 425288DEST_PATH_IMAGE016
Drain water, oven dry, sub-sieve makes the A material.
(2), amination reaction prepares the B material
Figure 536464DEST_PATH_IMAGE002
Press column weight amount (kilogram) and take by weighing following raw materials according, in clean reactor, add A material and tetraethylene pentamine, start stirring;
A material 380
Tetraethylene pentamine 1580
Figure 668849DEST_PATH_IMAGE004
Be warming up to 130-135 ℃, insulation reaction 15-18h, the control exchange is qualified greater than 8.0mmol/g in the survey;
Figure 823756DEST_PATH_IMAGE006
After middle control is qualified, take out mother liquor, reclaim tetraethylene pentamine;
Massive laundering is drained to neutral, gets the B material;
(3), methylation reaction prepares resin
2, operation steps
The B material is added in the mixing raw material of following weight part, start stirring;
Formic acid 1150-1250
Water 200-240
Formaldehyde 60-65
Oxalic acid 50-55
Figure 745947DEST_PATH_IMAGE004
Be warming up to 48-50 ℃, kept 20-40 minute;
Figure 822488DEST_PATH_IMAGE006
Drain mother liquor, massive laundering is drained discharging to neutral.
The ion exchange resin specific surface area that the present invention makes can reach 70m 2More than/the g, greater than 50%, complete exchange capacity reaches 11.8mmol/g greater than the mesopore ratio of 2nm.

Claims (1)

1. the preparation method of weakly alkaline TAIC anionite-exchange resin is characterized in that may further comprise the steps:
(1), polymerization prepares A material, may further comprise the steps:
Figure 46581DEST_PATH_IMAGE001
The water raw material that takes by weighing following weight part mixes, and stirs;
Deionized water 500-600
Gelatin 30-35
Walocel MT 20.000PV 50-60
Quadrol 15-20
Sodium-chlor 80-85
Sodium Persulfate 1-2
Be neutral with sulfuric acid water transfer phase PH
Figure 2012104898838100001DEST_PATH_IMAGE002
Take by weighing the raw material of following weight part, aqueous phase after adding after mixing is adjusted rotating speed depending on the granularity situation;
Methyl acrylate 32-34
Divinylbenzene 50-55
TAIC 270-290
200# gasoline 158-163
Clorafin 50-55
Ferrocene 8-12
Diisopropyl azodicarboxylate 3-5
Figure 337623DEST_PATH_IMAGE003
Slowly be warming up to 65-69 ℃, note observing spheroid granularity and typing situation;
Figure 2012104898838100001DEST_PATH_IMAGE004
Heat release during typing, cooling maintains the temperature at 68-70 ℃ after the heat release, be incubated 2-3 hour;
Figure 930410DEST_PATH_IMAGE005
Be warming up to 80-82 ℃ of insulation 3-4h with the 25-40 minutes;
Figure 2012104898838100001DEST_PATH_IMAGE006
With 92-96 ℃ of insulation of 50-70 minutes intensification 4-5h;
With the hot water wash nodule number all over till limpid to water;
Figure 2012104898838100001DEST_PATH_IMAGE008
Drain water, oven dry, sub-sieve makes the A material;
(2), amination reaction prepares the B material
Figure 392188DEST_PATH_IMAGE001
Press the row weight part and take by weighing following raw materials according, in clean reactor, add A material and tetraethylene pentamine, start stirring;
A expects 380-420
Tetraethylene pentamine 1580-1620
Be warming up to 130-135 ℃, insulation reaction 15-18h, the control exchange is qualified greater than 8.0mmol/g in the survey;
Figure 544001DEST_PATH_IMAGE003
After middle control is qualified, take out mother liquor, reclaim tetraethylene pentamine;
Figure 54486DEST_PATH_IMAGE004
Massive laundering is drained to neutral, gets the B material;
(3), methylation reaction prepares resin
2, operation steps
Figure 785681DEST_PATH_IMAGE001
The B material is added in the mixing raw material of following weight part, start stirring;
Formic acid 1150-1250
Water 200-240
Formaldehyde 60-65
Oxalic acid 50-55
Figure 592095DEST_PATH_IMAGE002
Be warming up to 48-50 ℃, kept 20-40 minute;
Figure 408741DEST_PATH_IMAGE003
Drain mother liquor, massive laundering is drained discharging to neutral.
CN201210489883.8A 2012-11-27 2012-11-27 The preparation method of weakly alkaline TAIC anionite-exchange resin Active CN103012676B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210489883.8A CN103012676B (en) 2012-11-27 2012-11-27 The preparation method of weakly alkaline TAIC anionite-exchange resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210489883.8A CN103012676B (en) 2012-11-27 2012-11-27 The preparation method of weakly alkaline TAIC anionite-exchange resin

Publications (2)

Publication Number Publication Date
CN103012676A true CN103012676A (en) 2013-04-03
CN103012676B CN103012676B (en) 2016-04-27

Family

ID=47961820

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210489883.8A Active CN103012676B (en) 2012-11-27 2012-11-27 The preparation method of weakly alkaline TAIC anionite-exchange resin

Country Status (1)

Country Link
CN (1) CN103012676B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1266690A2 (en) * 2001-06-04 2002-12-18 Rohm And Haas Company Preparation of weak acid cation exchange resins
CN102190753A (en) * 2010-03-19 2011-09-21 周家付 Preparation method for macroporous weak-acidic cation exchange resin
CN102189008A (en) * 2011-04-11 2011-09-21 常州大学 Novel strongly and weakly alkaline anion exchange resin and preparation method thereof
CN102671718A (en) * 2012-06-11 2012-09-19 淄博东大弘方化工有限公司 Supermacroporous strong base anion exchange resin with quaternary amine group and preparation process thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1266690A2 (en) * 2001-06-04 2002-12-18 Rohm And Haas Company Preparation of weak acid cation exchange resins
CN102190753A (en) * 2010-03-19 2011-09-21 周家付 Preparation method for macroporous weak-acidic cation exchange resin
CN102189008A (en) * 2011-04-11 2011-09-21 常州大学 Novel strongly and weakly alkaline anion exchange resin and preparation method thereof
CN102671718A (en) * 2012-06-11 2012-09-19 淄博东大弘方化工有限公司 Supermacroporous strong base anion exchange resin with quaternary amine group and preparation process thereof

Also Published As

Publication number Publication date
CN103012676B (en) 2016-04-27

Similar Documents

Publication Publication Date Title
CN103012644B (en) The preparation method of superacicd styrene system exchange resin
CN103008018B (en) The production method of storng-acid cation exchange resin
CN101781379A (en) Preparation method of D301 macroporous weekly acidic styrene type anion exchange resin
CN102050435B (en) Production method of battery-grade iron phosphate
CN102716770A (en) Method for preparing macropore strong acid cation exchange resin with high specific surface area
CN103008020B (en) Production method of strong-acid compound styrene cation exchange resin
CN102463155A (en) Method for preparing macroporous alkalescent anion exchange resin
CN103012658A (en) Production method for strongly basic anion exchange resin
CN103012645B (en) The production method of high exchange capacity superacicd styrene cation exchange resin
CN101759826A (en) Method for preparing D202 macroporous strong basic styrene series II type anion exchange resin
CN103008028A (en) Preparation method of alkalescent acrylic anion exchange resin
CN103012657A (en) Preparation method of macroporous slightly-alkaline acrylic acid composite TAIC anion exchange resin
CN103012676B (en) The preparation method of weakly alkaline TAIC anionite-exchange resin
CN109180851B (en) High-temperature-resistant guanidyl strong base resin and preparation method thereof
CN103008021B (en) Preparation method of large-exchange-capacity strong-alkaline acrylic anion exchange resin
CN103012654A (en) Production method of macroporous strongly-alkaline methyl acrylate anion exchange resin
CN103008024B (en) Preparation method of macroporous slightly-alkaline acrylonitrile anion exchange resin
CN103012653A (en) Process for preparing strong-basicity acrylic acid series anion exchange resin
CN101445573A (en) Method for preparing single-dispersibility polystyrene-DVE
CN103012681A (en) Production method of high-exchange-capacity macroporous strongly-alkaline acrylic acid series anion exchange resin
CN103008029A (en) Preparation method of macroporous weak-alkaline compound acrylic anion exchange resin
CN103012656A (en) Preparation method of macroporous weak-alkaline compound acrylic anion exchange resin
CN103012675A (en) Preparation method of macroporous weak-alkaline acrylic anion exchange resin
CN103012687A (en) Method for producing high-exchange-capacity strong acid styrene cation exchange resin
CN103012655A (en) Preparation method of large-exchange capacity slightly-alkaline acrylic acid series anion exchange resin

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant